HRID456140

反应详情

EQUATION

反应方程式

HRID 456140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a mixture of 6-((6-vinyl-1H-[1,2,3]triazolo[4,5-b]pyrazin-1-yl)methyl)quinoline (100 mg, 0.347 mmol) and 2,6-dimethylpyridine (74.3 mg, 0.694 mmol), was added a solution of osmium(VIII) oxide (297 mg, 1.387 mmol) in H2O (1.333 mL), followed by a solution of sodium periodate (88 mg, 6.94 μmol) in 1,4-Dioxane (4 ml). The reaction mixture was stirred at rt for 10 h. The solvents was removed in vacuo and DCM was added to dilute the residue. The resulting solution was washed with saturated NaHCO3, NH4Cl and brine. The organic layer was separated, dried over Na2SO4, and concentrated to give a crude product, which was purified with Analogix gel silica (Hexanes:EA) to afford 45 mg of title compound in 43% yield. LCMS (method B): [MH]+=291, tR=1.00 min.

WORKUP

后处理

  1. customThe solvents was removed in vacuo and DCM
  2. additionwas added
  3. additionto dilute the residue
  4. washThe resulting solution was washed with saturated NaHCO3, NH4Cl and brine
  5. customThe organic layer was separated
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated
  8. customto give a crude product, which
  9. customwas purified with Analogix gel silica (Hexanes:EA)